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ll iTEn STATES PATENT Eric,

JOHN H. STEVENS, OF NEWARK, NEW JERSEY, ASSIGNOR TO THE CELLUQ LOID MANUFACTURING COMPANY, OF NEW YORK, N. Y.

MANUFACTURE OF COMPOUNDS F PYROXYLINE OR NlTRO-CELLULOSE.

SPECIFICATION forming part of Letters Patent No. 269,341, dated December 19, 1882.

Application filed June 12, 1882. (No specimens.)

To all whom it may concern Be it known that I, JOHN H. STEVENS, of

the city of Newark, in the county of Essex and State of New Jersey, have invented cerrain new and useful Improvements in the Manutacture of Compounds of Pyroxyline or Nitro- Gellulose, ofwhich improvements the following I 1 soluble, (of which insoluble grades explosive gun-cotton is an exainple,) as my compounds are intended to be used in the manufacture of various articles formed by molding or shaping the compound in dies, or by cutting, carving,

I or turning it from a seasoned block or mass.

Heretot'ore such compounds have been made by dissolving the soluble nit-ro-cellulose with alcohol and ether, wood-naphtha, and other liquids which are active solventsof such nitro- 2 celluloseattheordinarytemperature; and camphor has been sometimes added to the compound either before or after the solution of the nitrocellulose by such active liquid solvents. lthas alsolong been known that camphor is of 0 itself an active solvent of nitro-eellnlose at the ordinary temperature when the camphor is dissolved in a inenstruum-sueh as alcohol or wood-naphtha orwheu acompound is formed of nitro-cellulose, camphor, and certain melt 5 strna which will liquefy the camphor whatever may be the order in which these ingredients are brought together. It is also well known that a mechanical mixture of intro-cellulose and camphor may be made and afterward subject- 0 ed to heat and pressure in closed dies, the

heat liquefying the camphor and thus developing its solvent action, the camphor being in such cases termed a latent solvent, by reason of its inaction until liquefied, whether by 5 heat or by a meustruum. The best practice has been found to demand the mixing of the camphor with the nitro-cellulose and then the addition to that compound of some liquid menstruum which, whi1e not actively developing the solvent power of the camphor, brings it into a softened condition, which facilitates its liquefaction under heat; and while numerous inenstrua have been employed in this way or suggested for this purpose, they have been heretofore, so far as 1 know, only used practically in conjunction with camphor and for the purpose ofliquefying or softening the camphor,

as above set forth.

Now, it is the objectofmyinvention to effect the solution, or, as it is more generally desig- 6o nated,the conversion of soluble nitro-cellulose by means of latent liquid solvents without necessarily employing cam phor in the compound; and by a seriesofexperiinents addressed to this end I have ascertained that this may be done in the following manner: The soluble nitro-cellulose should be groundintopulp and dehydrated by hydraulic pressure between absorbent pads, as is well understood. The dried nitro-cellnlose is then broken up into small pieces and placed in a vessel which can be tightly closed. To one part, by weight, of this intro-cellulose I add an equal quantity, by weigh t, of oil of garawayseed,onoil qtlryssop, dToil of sage or. .ofntansy oruoil .Qffil ies, oFoiFof winter-green, or of mixtures of these ousytinoration I have discovered to be a latent solvent of intro-cellulose, as hereinafter further explained. The latent liquid solvent being added to the pyroxyline, as above described, the box is tightly closed and the mixture is allowed to stand for, say,about twelve hours, or it may be stirred at intervals to effeet a more rapid and thorough absorption of the solvent by the nitro-cellulose,at the end of 8 which period it will. be louud that the nitrocellulose has been appreciably softened by the liquid solvent without any active development of the converting process. I then subject the mass to heavy pressure in glosed dies at a temo perature of about 200 Fahrenheit, and if it is tound necessary or desirable to repeat this pressing operation to more thoroughly complete the conversion I again break up the mass into small pieces, and put the compound again 5 in the dies and under heat and pressure, as 21-b0"6 described. I have found that the abovespecified oils operate in the same manner as camphor, in that they do not exert their solvent power prematurely,and by their use I am enabled to make a mechanical mixture in the first instances with the advantages of the suspension of the solvent action or converting operation, as is well understood, and then to complete the process by the application of heat and pressure, as above described.

With the nitro-cellulose and latent liquid solvents above specified Icompound such coloring-matters or inert substances as may be desired for any special purposes, and the products thus obtained are subjected to the ordinary seasoningoperation, after which they may be molded into shapes,in the ordinary manner, under heat and pressure. 1 subject the compound to heat and pressure in closed dies, as above stated, rather than in open rolls, as is customary in treating such compounds, because I have found that my new latent liquid solvents are better adapted to such treatment; but if I desire to treat the compoundsin open rolls or to develop the solvent power of the oils above mentioned at the ordinary temperature, it is only necessary to compound the ingredients as follows: To two parts, by weight, of nitro-cellulose I add two to three parts, by weight, of a mixture of one part, by Weight, of either of the oils above mentioned, or of any mixtureof those oils compounded together, as hereinbefore described, and two to three parts of alcohol or of wood-naphtha, and this will cause the developmentof the converting power of the solvent and effect the conversion of the niiro-cellulosc even in the cold or morerapidly in the ordinary masticating-rolls, and the product, if the seasoning operation has not been carried too far, will be susceptible of being remolded in the usual way.

Coloring-matter s and other inert substances maybe incorporated with the mixture of nitrocellulose and latent liquid solvent, and other substances may he added to impart any speciallydesired quality in the product. \Vith the latent liquid solvents above specified it will generally be found necessary to employ coloring-matters, as the compounds made with the above-specified oils are not well adapted for the manufacture of colorless or even of white material.

It will be seen that I have discovered certain latent liquid solvents which may be mechanically mixed with soluble nitrocellulose, and thus I am enabled to secure the advantages of a latent solvent and a preliminary mechanical mixture without the necessary intervention of any solid converting agentsuch as camphor; but it is an additional element of novelty as well as of utility in my improvements, that the use of these latent liquid solvents is entirely compatible with the use of camphor as well as with the use of active solventssuch as \vood'naphtha, or ether and alcohol. In other words, my new latent liquid solvents may be added in the hereinbeiore-described manner tocoinpouuds oi pyroxyline and camphor, with an enhancement of the solvent or converting action induced by the development of the latent solvent action of the camphor by the addition of the latent liquid solvent.

Having thus described the nature and ob- Witnesses:

WM. L. BnIcE, ABRAHAM M ANNERS. 

